Methods of chemical analysis for glass raw materials for colour picture tubes-Methods for chemical analysis for arenaceous quartz
Some standard content:
Electronic Industry Standard of the People's Republic of China SJ/1 10087. 1~~10087. 8—91
Chemical analysis methods for the main raw materials of color picture tube glass
Published on April 8, 1991
Implemented on July 1, 1991
Published by the Ministry of Machinery and Electronics Industry of the People's Republic of China Electronic Industry Standard of the People's Republic of China Chemical analysis methods for weak quartz
Methods far chemical analysis at zibiccous srkTSubject content and scope of application
1.1 Content
8J/T 10087. 1-9 [
This standard specifies the analysis method of quartz sand used as raw material for color picture tubes 1.2 Applicable scope
This standard applies to the routine analysis of quartz sand used as raw material for color picture tubes, and also applies to the analysis of quartz sand used as raw material for color picture tubes and other glass raw materials with relevant technical requirements, 25! Applicable standards
GB900D.1 General principles of analysis method for weakening of electrochemical performance
3.1 Analysis of single-shell
Code energy density sample 1.0 Store in a pot for 1000 years, cover with a thin film, first heat at low temperature, then gradually heat at high temperature, and finally place in a deep cold place! 15mlm weighed under 1230℃, the result is calculated by the following formula, average reduction (%) = * = * × 106
empty vortex disk S:
W, - test, 8:
, one-room for & I live shoot the amount
3.2 Analysis of silicon dioxide (water weight disk spectrophotometry, this side reaches the use of data protection analysis) 3.2.1 Test mix with the offer of culture, just acid solution. English: history of silicic acid dirty water. The same acid solution of the bottom of the disk. The sediment is applied, burned, and filled. Use the name of the building to completely drive out the carbon dioxide, from the reduction of the appropriate basis for the reduction of carbon dioxide, take the source of pollution, use the legal chemical life, the total amount of carbon dioxide in the sample and the liquid reagent 3.2.2
steep; 46%, 1.5;
Tongxin, the type of strong combustion rate of Keli Dian Du to remove the dangerous silicate with the protection of the plastic bottle. Salt 1191: 1:,:
Ministry of Electronic Industry of the People's Republic of China-4-1550701 implementation
Sulfuric acid::
dAnhydrous carbonate
SJ/T 10087.1-91
c. Preservation chain: K, stored in plastic bottle
1 Fine acid is more soluble: In%
Dissolve 10% of tartaric acid (N) M in water to make the volume Cm. If there is oil, it should be kept in the mold. If there is precipitation, prepare the new: 8% of tartaric acid:! tt||Dissolve 10% of tartaric acid in 100% of water and store in plastic. h. Anti-dissolution: Place the standard silicon dioxide with a concentration of 5.1m/ml in a single material cabinet, add 1g of carbon monoxide, run the valve fully, cool in water, move the water to the scale (0.100m). Ensure that the plastic is in good condition. Use twice the amount of water to accurately select 3.2.3 Sample
New test sample to see the test method to take out 20, grind it in a bowl (when rubbing lightly, there is no particle feeling! Don't worry 11 (constant short baking special level continuation? h, the material has been dried and cooled to the intersection of the exchange and said. 3.2.4 Steps
Accurately take the test sample and add 5 anhydrous carbonic acid to the blood, mix well, start heating at low temperature to avoid heating ~ 1 such as purchase roasting melt about rm, take out platinum, that is, the plate surface and cool: hydrochloric acid 203 is heated and dissolved on the edge, the surface of the water is strictly selected, and then collected, evaporated on the sand to nearly the card after the reduction of the film head ring 1-10 ml of iodine is added to the precipitate, and then heated in water for 5 minutes. The solution can be quickly dissolved. Add an appropriate amount of quantitative solution. Slowly reduce the amount, wash with a 1:50 hot plate, then use hot water to fully select the cloth, and make sure that the washing liquid is replenished within 30 minutes. The precipitate is not changed enough and put into the gold stack, add 1:1 acid to 1:1, and start to decompose the paper. Burn about 1-10 ml of paper cloth, cool it in a desiccator, and repeat the burning until the water shows diketone. Oxidize the starch, add 13 drops of 100 μl of hydrochloric acid and 10 μl of condensed water, add 3 ml of hydrochloric acid, and after the sugar alcohol is fully fermented, calculate at 103°C for 5 minutes, cool in a desiccator, weigh the cooled portion of the tablets received in the beaker, put it into a 25 ml volume, dilute with water to 0.5 ml, and absorb about 10 μl of the acid. Put it into the gelatin evenly. Place 5 ml of the right ascorbic acid solution in a 0.5 ml bottle and dilute with water to 0.5 ml. Place the solution in the left ventricle for 10 minutes. 65m absorbance, standard working curve: according to the ratio of the measured absorbance of the standard liquid 0.-0.0m (including oxidized C-0.50m) respectively in 100ml plastic environment to form a standard solution. Add 171 1m each, the following steps to make the relationship between the absorbance and the concentration of silicon dioxide as the working curve: 3.2.5 Calculation of the measured absorbance from the standard to determine the amount of silicon dioxide in the test solution, the following formula is used to calculate the content of silicon dioxide in the test solution:
In the formula: w, -
SJ/T 10087.1:97
S)=(W,-W)+eX 250/10
The mass of the precipitate and the precipitate before treatment with iodine-containing acid is 8:F, the mass of the precipitate and the precipitate after treatment with chlorinated ... Calculate the amount of silicon dioxide from the two weighings, and use the chromatographic method to determine the amount of silicon dioxide remaining in the sample. The sum of the two is the content of silicon monoxide in the sample. 3.3.2 Test and analysis Add 1% ethylene oxide to 207 mL of water, and dissolve it in 0.1% ethylene oxide while stirring. Store in a plastic bottle. It can be stored for a week. Other reagents and reagents are included in 3.2.2. 3.3.3 Test sample is the same as 3.2.3.
5.3.4 Analysis steps
Accurately weigh 0.5g of the sample and place it in a white gold evaporator. Add 1.5g of anhydrous sodium carbonate and 0.2g of sodium ether to the mixture. After eluting, heat it at low temperature and dissolve it at 1C00 for about 30 minutes. Collect the sample, cover it, cool it and add 20ml of 1% hydrochloric acid. Heat it in a water bath to dissolve it. Continue to heat it for about 20 minutes. Wash the surface with water, add an appropriate amount of quantitative filter paper, mix it evenly, add ethylene oxide for about 10 minutes, and mix it evenly. Dissolve it by about 5mm, filter it with slow quantitative filter paper, first precipitate it with 1150℃ hot hydrochloric acid, and then rinse it thoroughly with hot water. Collect the precipitate and put it in a 300mL beaker. Save it for the determination of the residual silicon in the filtrate.
Put the precipitate and paper in the vortex, add 1:1 acid 2~-8, low temperature sintering, heat at 1000-1100℃ for about 60min, put in the dryer, weigh. Repeat the sintering until the amount is less, the determination of silicon dioxide in the slurry is the same as the wide operation of silicon dioxide in the filter source in 3.2.4. Note: 1) The melting is not true, otherwise the plate is difficult to solve. 3.35 Calculation of the results of analysis
No residual silicon dioxide is continuously produced on the working curve. The content of silicon dioxide in the sample is calculated by formula (2). 5.56 Precision
The relative standard deviation is less than 0.15%. 3.4 Analysis of silica (mixing method) 3.4.1 Method Summary This method is applicable to the analysis of silica containing more than 99.1 trillion. The sample is treated with nitric acid to remove all silica. The difference in mass before and after treatment is used to calculate the content of silica. 34.2 Reagents and standards Electrochemical aldehyde, high-grade pure, b. sulfuric acid; I.1, 3.4.3 Same as 8.2.3. 3.4.4 Analytical procedures SI/T 10087.1-91 Weigh the sample 1.In the platinum vaporized blood that has been plated, add a little ice source, such as 15 ml of chlorinated acid, 1:1, 1:1, put it on a sand bath, evaporate until white smoke begins to appear. Remove it, add chlorine, cool it to a plate, use a little water to blow the inner wall of the blood, then add 5 ml of chlorine and evaporate it to the bottom of the cover in a muffle furnace at 1000 ℃ for 30 minutes. The material is taken to the room and weighed.
3.4.5 Analysis and calculation
The following formula is used to calculate the silicon content in the sample and the product:
The residual platinum after hydrochloric acid treatment is different from the original! The sample volume is, 5.4.6 The density and the relative standard deviation are adjusted to 0.1%, 3.5 Analysis of ferrous oxide and ferric oxide 3.5.7 After the sample is treated with hydrogen chlorine, hydrogen peroxide and silicon dioxide is removed, it is dissolved in a neutral acid medium and determined by the absorption method. 3.5.2 Reagents and solutions Hydrogen fluoride, nitric acid, 1 Strontium nitrate concentration: 10%: Standard aluminum oxide: 5 cumk/ml, Standard ferric oxide: 220 mB/ml 3.5.3 Instrument and its working parts Absorption spectrophotometer. Hollow pole lamp.
Instrument. 1. Operating conditions are shown in Table.
Table 1. Setting of Japanese A-610-13 atomic absorption spectrometer. Operating conditions
. 5. 4 Sample
3. 2. 3.
Normal wavelength
Preferred electric current
Preferred burner
Gas type
Normal gas
Air-acetylene
Quantity, J, mln
3.5.5 Analysis procedure
SJ/T IC087. 1—91
. After the leakage is confirmed, take a sample of 1-20 ml of blood, add a little water, add 5M high-purity acid, 0.04% oxygen, and slowly float on the sand. After cooling, rinse the whole body with a little water and add oxygen for 20 minutes. Add nitric acid solution, transfer to a 10-ml mother bottle after cooling, add 1M nitric acid solution, stir well and then dilute with water. Follow the same steps as the main sample operation steps to empty the test solution. Put the test solution and the white liquid into the table! The instrument working system is set, and the atomic mass spectrometry of lead and iron is determined.
Low light support 2 requirements to prepare alumina, ferric oxide standard series, according to the working conditions, formulate the standard series of aluminum, coin atomic absorption related substances, and give the relationship between the energy and absorption of aluminum and coin trioxide as the working property line,
Table 2 Alumina, lead sesquioxide, ferric oxide standard series solution
Introduce the tour,
Calcium sesquioxide standard solution
|Tri-iron oxide liquid, 20 yuan
job":
3-5.E Calculation of analysis results
3.5. The sample liquid obtained by the system is absorbed by the liquid. The corresponding amount of ferric oxide and iron oxide is found from the working curve respectively, and the total amount of ferric oxide and iron oxide in the test library is calculated by the following formula: M(%)=
In practice: MO (drug)
(.1 - 4.) × 10)
The percentage of the new sample (trioxide) in one year: A—the ratio of lead trioxide to titanium trioxide in the sample economy is 1.2; the sample is checked from the 1 action line. The precision is less than 3. 6. 7. The error is less than the standard. The difference between the three grams of trioxide and the standard is less than 1. 2 ... 11
High-purity acid solution: C.551
Pressure solution: 23%bzxZ.net
Material acid oil solution:
SI/T10087.1--91
Ferric sulfate solution: containing 1mg/ml
g diphenylcarbazide solution: U.2-hydroxy- ... 3.8.4 Analytical steps: 1. Place the confirmed sample 2.D52 in a preheated oven and add 15 ml of hydrochloric acid and 4 ml of 1:1 magnetic acid. Heat in a water bath to decompose. Heat until the fumes of the magnetic acid begin to emit. After cooling, continue heating in a water bath for 15 minutes and then stop the fumes. Cool and add 1 ml of anti-aldehyde and water. Heat in a water bath for about 2 minutes. During the washing process, filter and wash at high speed 7 to 8 times at high temperature, then add 1ml of acid solution into a beaker with water to 7ml. Add 2ml of potassium permanganate and continue boiling until the liquid is about 1. After cooling, add 20 drops of new 10% sodium hyaluronate solution and stir until the red color of the egg white disappears.
e. Transfer this liquid into a 1m2 plate, add distilled water and irradiate it with water until it develops color:
f.5m later, take a 2cm drop of this colorimetric solution at a colorimetric grid near 50° length and measure it with an isophotometer. Use water as the reference.
Preparation of standard curve: Pipette lead series solution, and place it in F200 standard water at a concentration of about 3:1 for 5m, and proceed as follows according to the analysis of 3.1:1 for a~. According to the standard series of data, the absorption and light pressure are plotted, and the large series of chromium trioxide content and photometry are used as the standard analysis line. 3.6.5 Calculation of analysis results. According to the absorbance obtained by the test wave, the standard is used to calculate the "chromium trioxide content" in the sample according to the following formula. Cno63>=WX:6n × 100. The sample content is 8.
3.G6.
The difference between the standard and the standard is less than %.
Additional instructions:
This standard is the responsibility of the Ministry of Machinery and Electronics Industry! This standard is drafted by the Ministry of Machinery and Electronics Industry and the North China Institute of Electronics. The main drafters of this standard are Guanghui, Yongsoft,1—91
. After the leakage is confirmed, take a sample of 1~20 ml from the blood, add a little water and then add 5m high acid, 0.04% oxygen, and slowly float on the sand. After cooling, rinse the whole body with a little water and add oxygen for 20 minutes. Add nitric acid and dissolve it in a sand bath until it is completely cooled. Add 1m nitric acid solution and transfer it to a mother bottle. After cooling, add 1m nitric acid solution and stir well. Then dilute it with water until it is diluted.
Follow the steps described above for the sample operation. Put the test solution and the white liquid into the blank according to the table! The instrument working system is set, and the atomic mass spectrometry of lead and iron is determined.
Low light support 2 requirements to prepare alumina, ferric oxide standard series, according to the working conditions, formulate the standard series of aluminum, coin atomic absorption related substances, and give the relationship between the energy and absorption of aluminum and coin trioxide as the working property line,
Table 2 Alumina, lead sesquioxide, ferric oxide standard series solution
Introduce the tour,
Calcium sesquioxide standard solution
|Tri-iron oxide liquid, 20 yuan
job":
3-5.E Calculation of analysis results
3.5. The sample liquid obtained by the system is absorbed by the liquid. The corresponding amount of ferric oxide and iron oxide is found from the working curve respectively, and the total amount of ferric oxide and iron oxide in the test library is calculated by the following formula: M(%)=
In practice: MO (drug)
(.1 - 4.) × 10)
The percentage of the new sample (trioxide) in one year: A—the ratio of lead trioxide to titanium trioxide in the sample economy is 1.2; the sample is checked from the 1 action line. The precision is less than 3. 6. 7. The error is less than the standard. The difference between the three grams of trioxide and the standard is less than 1. 2 ... 11
High-purity acid solution: C.551
Pressure solution: 23%
Material acid oil solution:
SI/T10087.1--91
Ferric sulfate solution: containing 1mg/ml
g diphenylcarbazide solution: U.2-hydroxy- ... 3.8.4 Analytical steps: 1. Place the confirmed sample 2.D52 in a preheated oven and add 15 ml of hydrochloric acid and 4 ml of 1:1 magnetic acid. Heat in a water bath to decompose. Heat until the fumes of the magnetic acid begin to emit. After cooling, continue heating in a water bath for 15 minutes and then stop the fumes. Cool and add 1 ml of anti-aldehyde and water. Heat in a water bath for about 2 minutes. During the washing process, filter and wash at high speed 7 to 8 times at high temperature, then add 1ml of acid solution into a beaker with water to 7ml. Add 2ml of potassium permanganate and continue boiling until the liquid is about 1. After cooling, add 20 drops of new 10% sodium hyaluronate solution and stir until the red color of the egg white disappears.
e. Transfer this liquid into a 1m2 plate, add distilled water and irradiate it with water until it develops color:
f.5m later, take a 2cm drop of this colorimetric solution at a colorimetric grid near 50° length and measure it with an isophotometer. Use water as the reference.
Preparation of standard curve: Pipette lead series solution, and place it in F200 standard water at a concentration of about 3:1 for 5m, and proceed as follows according to the analysis of 3.1:1 for a~. According to the standard series of data, the absorption and light pressure are plotted, and the large series of chromium trioxide content and photometry are used as the standard analysis line. 3.6.5 Calculation of analysis results. According to the absorbance obtained by the test wave, the standard is used to calculate the "chromium trioxide content" in the sample according to the following formula. Cno63>=WX:6n × 100. The sample content is 8.
3.G6.
The difference between the standard and the standard is less than %.
Additional instructions:
This standard is the responsibility of the Ministry of Machinery and Electronics Industry! This standard is drafted by the Ministry of Machinery and Electronics Industry and the North China Institute of Electronics. The main drafters of this standard are Guanghui, Yongsoft,1—91
. After the leakage is confirmed, take a sample of 1~20 ml from the blood, add a little water and then add 5m high acid, 0.04% oxygen, and slowly float on the sand. After cooling, rinse the whole body with a little water and add oxygen for 20 minutes. Add nitric acid and dissolve it in a sand bath until it is completely cooled. Add 1m nitric acid solution and transfer it to a mother bottle. After cooling, add 1m nitric acid solution and stir well. Then dilute it with water until it is diluted.
Follow the steps described above for the sample operation. Put the test solution and the white liquid into the blank according to the table! The instrument working system is set, and the atomic mass spectrometry of lead and iron is determined.
Low light support 2 requirements to prepare alumina, ferric oxide standard series, according to the working conditions, formulate the standard series of aluminum, coin atomic absorption related substances, and give the relationship between the energy and absorption of aluminum and coin trioxide as the working property line,
Table 2 Alumina, lead sesquioxide, ferric oxide standard series solution
Introduce the tour,
Calcium sesquioxide standard solution
|Tri-iron oxide liquid, 20 yuan
job":
3-5.E Calculation of analysis results
3.5. The sample liquid obtained by the system is absorbed by the liquid. The corresponding amount of ferric oxide and iron oxide is found from the working curve respectively, and the total amount of ferric oxide and iron oxide in the test library is calculated by the following formula: M(%)=
In practice: MO (drug)
(.1 - 4.) × 10)
The percentage of the new sample (trioxide) in one year: A—the ratio of lead trioxide to titanium trioxide in the sample economy is 1.2; the sample is checked from the 1 action line. The precision is less than 3. 6. 7. The error is less than the standard. The difference between the three grams of trioxide and the standard is less than 1. 2 ... 11
High-purity acid solution: C.551
Pressure solution: 23%
Material acid oil solution:
SI/T10087.1--91
Ferric sulfate solution: containing 1mg/ml
g diphenylcarbazide solution: U.2-hydroxy- ... 3.8.4 Analytical steps: 1. Place the confirmed sample 2.D52 in a preheated oven and add 15 ml of hydrochloric acid and 4 ml of 1:1 magnetic acid. Heat in a water bath to decompose. Heat until the fumes of the magnetic acid begin to emit. After cooling, continue heating in a water bath for 15 minutes and then stop the fumes. Cool and add 1 ml of anti-aldehyde and water. Heat in a water bath for about 2 minutes. During the washing process, filter and wash at high speed 7 to 8 times at high temperature, then add 1ml of acid solution into a beaker with water to 7ml. Add 2ml of potassium permanganate and continue boiling until the liquid is about 1. After cooling, add 20 drops of new 10% sodium hyaluronate solution and stir until the red color of the egg white disappears.
e. Transfer this liquid into a 1m2 plate, add distilled water and irradiate it with water until it develops color:
f.5m later, take a 2cm drop of this colorimetric solution at a colorimetric grid near 50° length and measure it with an isophotometer. Use water as the reference.
Preparation of standard curve: Pipette lead series solution, and place it in F200 standard water at a concentration of about 3:1 for 5m, and proceed as follows according to the analysis of 3.1:1 for a~. According to the standard series of data, the absorption and light pressure are plotted, and the large series of chromium trioxide content and photometry are used as the standard analysis line. 3.6.5 Calculation of analysis results. According to the absorbance obtained by the test wave, the standard is used to calculate the "chromium trioxide content" in the sample according to the following formula. Cno63>=WX:6n × 100. The sample content is 8.
3.G6.
The difference between the standard and the standard is less than %.
Additional instructions:
This standard is the responsibility of the Ministry of Machinery and Electronics Industry! This standard is drafted by the Ministry of Machinery and Electronics Industry and the North China Institute of Electronics. The main drafters of this standard are Guanghui, Yongsoft,The following is carried out according to the analysis of 3..1 a~. According to the standard series of data, the absorption and light pressure are plotted, and the large series of chromium trioxide content and photometry are used as the standard analysis line. 3.6.5 Calculation of analysis results. According to the absorbance obtained by the test wave, the standard is used to calculate the "chromium trioxide content" in the sample according to the following formula. Cno63>=WX:6n × 100. The sample content is 8.
3.G6.
The difference between the standard and the standard is less than %.
Additional instructions:
This standard is the responsibility of the Ministry of Machinery and Electronics Industry! This standard is drafted by the Ministry of Machinery and Electronics Industry and the North China Institute of Electronics. The main drafters of this standard are Guanghui, Yongsoft,The following is carried out according to the analysis of 3..1 a~. According to the standard series of data, the absorption and light pressure are plotted, and the large series of chromium trioxide content and photometry are used as the standard analysis line. 3.6.5 Calculation of analysis results. According to the absorbance obtained by the test wave, the standard is used to calculate the "chromium trioxide content" in the sample according to the following formula. Cno63>=WX:6n × 100. The sample content is 8.
3.G6.
The difference between the standard and the standard is less than %.
Additional instructions:
This standard is the responsibility of the Ministry of Machinery and Electronics Industry! This standard is drafted by the Ministry of Machinery and Electronics Industry and the North China Institute of Electronics. The main drafters of this standard are Guanghui, Yongsoft,
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